CN113979768A - High-conductivity carbon electrode material and preparation method thereof - Google Patents
High-conductivity carbon electrode material and preparation method thereof Download PDFInfo
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- CN113979768A CN113979768A CN202111243702.9A CN202111243702A CN113979768A CN 113979768 A CN113979768 A CN 113979768A CN 202111243702 A CN202111243702 A CN 202111243702A CN 113979768 A CN113979768 A CN 113979768A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 65
- 239000007772 electrode material Substances 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 229910021382 natural graphite Inorganic materials 0.000 claims abstract description 74
- 239000002994 raw material Substances 0.000 claims abstract description 65
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims abstract description 64
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 44
- 239000004917 carbon fiber Substances 0.000 claims abstract description 44
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 37
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims abstract description 35
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229940112669 cuprous oxide Drugs 0.000 claims abstract description 35
- 239000004305 biphenyl Substances 0.000 claims abstract description 32
- 235000010290 biphenyl Nutrition 0.000 claims abstract description 32
- 239000011230 binding agent Substances 0.000 claims abstract description 30
- 238000005087 graphitization Methods 0.000 claims abstract description 11
- 239000004642 Polyimide Substances 0.000 claims description 28
- 239000011280 coal tar Substances 0.000 claims description 28
- 229920001721 polyimide Polymers 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 12
- 239000011261 inert gas Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 238000007873 sieving Methods 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000005229 chemical vapour deposition Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 239000003575 carbonaceous material Substances 0.000 claims 1
- 239000011159 matrix material Substances 0.000 abstract description 13
- 239000012744 reinforcing agent Substances 0.000 abstract description 9
- 239000000835 fiber Substances 0.000 abstract description 3
- 238000005303 weighing Methods 0.000 description 10
- 238000000498 ball milling Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 238000004898 kneading Methods 0.000 description 6
- 238000000465 moulding Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 2
- 239000005997 Calcium carbide Substances 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- CLZWAWBPWVRRGI-UHFFFAOYSA-N tert-butyl 2-[2-[2-[2-[bis[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]amino]-5-bromophenoxy]ethoxy]-4-methyl-n-[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]anilino]acetate Chemical compound CC1=CC=C(N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)C(OCCOC=2C(=CC=C(Br)C=2)N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)=C1 CLZWAWBPWVRRGI-UHFFFAOYSA-N 0.000 description 1
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a high-conductivity carbon electrode material and a preparation method thereof, wherein the mass ratio of a carbonaceous raw material to a binder is (5-10): 1; the carbon raw material comprises natural graphite, carbon fiber, biphenyl and cuprous oxide, the mass of the carbon fiber is 5-10% of the total mass of the carbon raw material, the mass of the biphenyl is 5-10% of the total mass of the carbon raw material, the mass of the cuprous oxide is 2-5% of the total mass of the carbon raw material, the balance is the natural graphite, the carbon fiber is used as a reinforcing agent, the natural graphite is used as a matrix of a carbon electrode, a carbon matrix is provided and is mixed with the biphenyl and the cuprous oxide according to a proportion, the carbon fiber is a conductive reinforcing agent and is used for improving the conductivity of the carbon matrix, a needle-shaped structure and fiber textures in the natural graphite are mixed with the carbon fiber as the reinforcing agent, the natural graphite and the carbon fiber are stabilized by using a binder, the cuprous oxide is a natural graphitization promoter to promote natural graphitization of a sample at high temperature, so that the conductivity is enhanced, and the non-volatile carbon of the natural graphite part, forming high-power and ultrahigh-power natural graphite electrodes.
Description
Technical Field
The invention belongs to the field of electrodes, and particularly relates to a high-conductivity carbon electrode material and a preparation method thereof.
Background
The industrial carbon electrode is widely applied to industry as an important conductive material, has the characteristic of wide application field compared with other carbon products, and can be used on smelting submerged arc furnaces of industrial silicon, yellow phosphorus, calcium carbide, iron alloy and the like. Since the resistivity of the carbon electrode is high, a large amount of power is consumed and the electrode is used, and therefore, how to reduce the resistivity of the carbon electrode is a major concern in the industry.
Disclosure of Invention
The invention aims to provide a high-conductivity carbon electrode material and a preparation method thereof, so as to overcome the defects of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-conductivity carbon electrode material comprises a carbonaceous raw material and a binder, wherein the mass ratio of the carbonaceous raw material to the binder is (5-10): 1; the carbonaceous raw material comprises natural graphite, carbon fiber, biphenyl and cuprous oxide, wherein the mass of the carbon fiber is 5-10% of the total mass of the carbonaceous raw material, the mass of the biphenyl is 5-10% of the total mass of the carbonaceous raw material, the mass of the cuprous oxide is 2-5% of the total mass of the carbonaceous raw material, and the balance is the natural graphite.
Further, the binder comprises coal tar and polyimide, and the mass ratio of the coal tar to the polyimide is 1: (0.5-2).
Furthermore, the particle size of the natural graphite is less than 150 meshes.
A preparation method of a high-conductivity carbon electrode comprises the following steps:
s1, taking a carbonaceous raw material and a binder, wherein the mass ratio of the carbonaceous raw material to the binder is (5-10): 1; the carbonaceous raw material comprises natural graphite, carbon fiber, biphenyl and cuprous oxide, wherein the mass of the carbon fiber is 5-10% of the total mass of the carbonaceous raw material, the mass of the biphenyl is 5-10% of the total mass of the carbonaceous raw material, the mass of the cuprous oxide is 2-5% of the total mass of the carbonaceous raw material, and the balance is the natural graphite;
s2, calcining natural graphite in an inert gas atmosphere, crushing and grinding the calcined natural graphite, sieving the crushed and ground natural graphite with a 150-mesh sieve, and uniformly mixing carbon fibers, biphenyl and cuprous oxide with the natural graphite sieved with the 150-mesh sieve to form a carbonaceous raw material;
and S3, uniformly mixing the carbonaceous raw material and the binder, and naturally graphitizing in a grinding tool to obtain the carbon electrode.
Further, nitrogen or argon is used as the inert gas.
Furthermore, calcining the natural graphite in an inert gas atmosphere to reduce volatile components and moisture in the natural graphite, wherein the calcining temperature is 1100-1300 ℃, and the heating time is 2-4 h.
Further, the carbon fiber, the biphenyl, the cuprous oxide and the natural graphite powder are ball-milled in a ball mill for not less than 30 minutes to form the carbonaceous raw material.
Further, the binder comprises coal tar and polyimide, and the mass ratio of the coal tar to the polyimide is 1: (0.5-2).
Further, the carbonaceous raw material and the binder are uniformly mixed and then are put into a mould, and are roasted for 2 to 3 hours at the temperature of 1200-1400 ℃, and the roasted raw material is naturally graphitized in a natural graphitization furnace at the temperature of 2700 to 2900 ℃ for 40 to 50 hours.
Furthermore, the carbon fiber is prepared by adopting a chemical vapor deposition method.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention relates to a high-conductivity carbon electrode material, which comprises a carbonaceous raw material and a binder, wherein the mass ratio of the carbonaceous raw material to the binder is (5-10): 1; the carbon raw material comprises natural graphite, carbon fiber, biphenyl and cuprous oxide, the mass of the carbon fiber is 5-10% of the total mass of the carbon raw material, the mass of the biphenyl is 5-10% of the total mass of the carbon raw material, the mass of the cuprous oxide is 2-5% of the total mass of the carbon raw material, the balance is the natural graphite, the carbon fiber is used as a reinforcing agent, the natural graphite is used as a matrix of a carbon electrode, a carbon matrix is provided and is mixed with the biphenyl and the cuprous oxide according to a proportion, the carbon fiber is a conductive reinforcing agent and is used for improving the conductivity of the carbon matrix, a needle-shaped structure and fiber textures in the natural graphite are mixed with the carbon fiber as the reinforcing agent, the natural graphite and the carbon fiber are stabilized by using a binder, the cuprous oxide is a natural graphitization promoter to promote natural graphitization of a sample at high temperature, so that the conductivity is enhanced, and the non-volatile carbon of the natural graphite part, forming high-power and ultrahigh-power natural graphite electrodes.
The invention relates to a preparation method of a high-conductivity carbon electrode, which comprises the steps of calcining natural graphite in an inert gas atmosphere to improve the chemical stability of the natural graphite, crushing and grinding the calcined natural graphite into powder, sieving the powder by a 150-mesh sieve, uniformly mixing carbon fibers, biphenyl and cuprous oxide with the natural graphite sieved by the 150-mesh sieve to form a carbonaceous raw material, taking the natural graphite as a matrix of the carbon electrode, providing a carbon matrix, mixing the carbon matrix with the biphenyl and the cuprous oxide according to a proportion, increasing the carbon fibers to improve the conductivity of the carbon matrix, uniformly mixing the carbonaceous raw material with a binder, and performing natural graphitization in a grinding tool to improve the stability of the high-conductivity carbon electrode.
Detailed Description
The invention is described in further detail below:
a high-conductivity carbon electrode material comprises a carbonaceous raw material and a binder, wherein the mass ratio of the carbonaceous raw material to the binder is (5-10): 1, the carbonaceous raw material comprises natural graphite, carbon fiber, biphenyl and cuprous oxide, the mass of the carbon fiber is 5-10% of the total mass of the carbonaceous raw material, the mass of the biphenyl is 5-10% of the total mass of the carbonaceous raw material, the mass of the cuprous oxide is 2-5% of the total mass of the carbonaceous raw material, the balance is natural graphite, the carbon fiber is used as a reinforcing agent, the natural graphite is used as a matrix of a carbon electrode, a carbon matrix is provided and is mixed with the biphenyl and the cuprous oxide according to a proportion, the carbon fiber is a conductive reinforcing agent and is used for improving the conductivity of the carbon matrix, a needle-shaped structure and fiber textures in the natural graphite are mixed with the carbon fiber as the reinforcing agent, the natural graphite and the carbon fiber are stabilized by using a binder, the cuprous oxide is a natural graphitization promoter, natural graphitization of a sample at high temperature is promoted, so that the conductivity is enhanced, and part of the natural graphite contains non-volatile carbon, the high-power and ultrahigh-power natural graphite electrode is formed, is completely different from artificial graphite, and carbon in non-natural graphite is completely volatilized after being heated, so that the performance of the graphite electrode is reduced.
The binder comprises coal tar and polyimide, and the mass ratio of the coal tar to the polyimide is 1: (0.5-2).
The particle size of the natural graphite is less than 150 meshes.
The preparation method of the high-conductivity carbon electrode based on the high-conductivity carbon electrode material comprises the following steps:
s1, taking natural graphite, carbon fibers, biphenyl, cuprous oxide, coal tar and polyimide according to the mass ratio, wherein the mass of the carbon fibers is 5-10% of the total mass of the carbonaceous raw materials, the mass of the biphenyl is 5-10% of the total mass of the carbonaceous raw materials, the mass of the cuprous oxide is 2-5% of the total mass of the carbonaceous raw materials, and the mass ratio of the coal tar to the polyimide is 1: (0.5-2); the mixing mass ratio of the carbonaceous raw material to the binder is (5-10): 1;
s2, calcining natural graphite in an inert gas atmosphere, crushing and grinding the calcined natural graphite, sieving the crushed and ground natural graphite with a 150-mesh sieve, and uniformly mixing carbon fiber, biphenyl, cuprous oxide and the natural graphite powder to form a carbonaceous raw material;
s3, heating and mixing the coal tar and the polyimide to form a binder;
and S4, uniformly mixing the carbonaceous raw material and the binder, and naturally graphitizing in a grinding tool to obtain the carbon electrode.
Specifically, the inert gas is nitrogen or argon; calcining natural graphite in an inert gas atmosphere to reduce volatile components and moisture in the natural graphite, wherein the calcining temperature is 1100-1300 ℃, and the heating time is 2-4 h; the total mass resistivity after being calcined at 1100 ℃ and 1300 ℃ is reduced to about 500 mu omega m, so that the conductivity is improved;
specifically, carbon fibers, biphenyl, cuprous oxide and natural graphite powder are subjected to ball milling in a ball mill for no less than 30 minutes to form a carbonaceous raw material; preparing the carbon fiber by adopting a chemical vapor deposition method to obtain the carbon nanofiber modified material.
The natural graphitization process comprises the following steps: uniformly mixing a carbonaceous raw material and a binder, putting the mixture into a mold, roasting the mixture for 2 to 3 hours at the temperature of 1200-1400 ℃, and naturally graphitizing the roasted raw material in a natural graphitization furnace at the temperature of 2700 to 2900 ℃ for 40 to 50 hours. And then cooling the obtained carbon electrode, taking out and carrying out performance measurement.
Example 1:
weighing 200g of natural graphite, calcining under the protection of nitrogen at 1100 ℃ for 2h, crushing and grinding the calcined natural graphite, and sieving by using a 150-mesh sieve. Taking 10g of three-dimensional oriented carbon fiber, 10g of biphenyl and 4g of cuprous oxide, ball-milling in a ball mill for 30 minutes, and uniformly mixing with natural graphite. And weighing 40g of a mixture of coal tar and polyimide in another beaker (the ratio of the coal tar to the polyimide is 1: 0.5), mixing the coal tar and the polyimide, kneading the mixture in a kneader, pouring the mixture into a mold for molding, roasting the roasted raw materials at 2700 ℃ for 44 hours, cooling to obtain a carbon electrode, and measuring the performance of the carbon electrode: resistivity of 7.8. mu. omega. m, and density of 1.63g/cm3。
Example 2:
weighing 200g of natural graphite, calcining under the protection of nitrogen at 1150 ℃ for 2.5h, crushing and grinding the calcined natural graphite, and sieving by using a 150-mesh sieve. Taking 12g of three-dimensional oriented carbon fiber, 10g of biphenyl and 5g of cuprous oxide, ball-milling in a ball mill for 30 minutes, and uniformly mixing with natural graphite. Weighing 35g of a mixture of coal tar and polyimide in another beaker (the ratio of the coal tar to the polyimide is 1: 1), mixing the coal tar and the polyimide, kneading the mixture in a kneading machine, pouring the mixture into a mold for molding, roasting the raw materials at 2800 ℃ for 48 hours, cooling to obtain a carbon electrode, and measuring the performance of the carbon electrode: resistivity of 6.1 μ Ω · m, and density of 1.55g/cm3。
Example 3:
weighing 200g of natural graphite, calcining under the protection of nitrogen at 1300 ℃ for 3h, crushing and grinding the calcined natural graphite, and sieving by using a 150-mesh sieve. Taking 13g of three-dimensional oriented carbon fiber, 11g of biphenyl and 5.5g of cuprous oxide, ball-milling in a ball mill for 30 minutes, and uniformly mixing with natural graphite. Weighing 33g of a mixture of coal tar and polyimide in a beaker (the ratio of the coal tar to the polyimide is 1: 1), mixing the coal tar and the polyimide, kneading the mixture in a kneader, pouring the mixture into a mold for molding, roasting the raw materials at 2900 ℃ for 45 hours, cooling to obtain a carbon electrode, and measuring the performance of the carbon electrode: the resistivity was 5.1. mu. omega. m, and the density was 1.58g/cm3。
Example 4:
weighing 200g of natural graphite under the protection of nitrogenCalcining at 1300 deg.C for 3 hr, pulverizing calcined natural graphite, and sieving with 150 mesh sieve. Taking 13g of three-dimensional oriented carbon fiber, 13g of biphenyl and 7g of cuprous oxide, ball-milling in a ball mill for 30 minutes, and uniformly mixing with natural graphite. Weighing 29g of a mixture of coal tar and polyimide in another beaker (the ratio of the coal tar to the polyimide is 1: 1), mixing the coal tar and the polyimide, kneading the mixture in a kneader, pouring the mixture into a mold for molding, roasting the raw materials at 2750 ℃ for 48 hours, cooling to obtain a carbon electrode, and measuring the performance of the carbon electrode: resistivity of 6.3. mu. omega. m, and density of 1.61g/cm3。
Example 5:
weighing 200g of natural graphite, calcining under the protection of nitrogen, crushing and grinding the calcined natural graphite, and sieving by using a 150-mesh sieve. Taking 18g of three-dimensional oriented carbon fiber, 18g of biphenyl and 9g of cuprous oxide, ball-milling in a ball mill for 30 minutes, and uniformly mixing with natural graphite. Weighing 29g of a mixture of coal tar and polyimide in a beaker (the ratio of the coal tar to the polyimide is 1: 2), mixing the coal tar and the polyimide, kneading the mixture in a kneader, pouring the mixture into a mold for molding, roasting the raw materials at 2850 ℃ for 50 hours, cooling to obtain a carbon electrode, and measuring the performance of the carbon electrode: the resistivity was 5, 7. mu. omega. m, and the density was 1.64g/cm3。
Claims (10)
1. The high-conductivity carbon electrode material is characterized by comprising a carbonaceous raw material and a binder, wherein the mass ratio of the carbonaceous raw material to the binder is (5-10): 1; the carbonaceous raw material comprises natural graphite, carbon fiber, biphenyl and cuprous oxide, wherein the mass of the carbon fiber is 5-10% of the total mass of the carbonaceous raw material, the mass of the biphenyl is 5-10% of the total mass of the carbonaceous raw material, the mass of the cuprous oxide is 2-5% of the total mass of the carbonaceous raw material, and the balance is the natural graphite.
2. The high-conductivity carbon electrode material as claimed in claim 1, wherein the binder comprises coal tar and polyimide, and the mass ratio of coal tar to polyimide is 1: (0.5-2).
3. The high-conductivity carbon electrode material as claimed in claim 1, wherein the natural graphite has a particle size of less than 150 mesh.
4. A preparation method of a high-conductivity carbon electrode is characterized by comprising the following steps:
s1, taking a carbonaceous raw material and a binder, wherein the mass ratio of the carbonaceous raw material to the binder is (5-10): 1; the carbonaceous raw material comprises natural graphite, carbon fiber, biphenyl and cuprous oxide, wherein the mass of the carbon fiber is 5-10% of the total mass of the carbonaceous raw material, the mass of the biphenyl is 5-10% of the total mass of the carbonaceous raw material, the mass of the cuprous oxide is 2-5% of the total mass of the carbonaceous raw material, and the balance is the natural graphite;
s2, calcining natural graphite in an inert gas atmosphere, crushing and grinding the calcined natural graphite, sieving the crushed and ground natural graphite with a 150-mesh sieve, and uniformly mixing carbon fibers, biphenyl and cuprous oxide with the natural graphite sieved with the 150-mesh sieve to form a carbonaceous raw material;
and S3, uniformly mixing the carbonaceous raw material and the binder, and naturally graphitizing in a grinding tool to obtain the carbon electrode.
5. The method for preparing a high-conductivity carbon electrode according to claim 4, wherein the inert gas is nitrogen or argon.
6. The method as claimed in claim 4, wherein the natural graphite is calcined in an inert gas atmosphere to reduce volatile components and moisture therein, the calcination temperature is 1100-1300 ℃, and the heating time is 2-4 h.
7. The method for preparing a high-conductivity carbon electrode according to claim 4, wherein the carbon fibers, the biphenyl, the cuprous oxide and the natural graphite powder are ball-milled in a ball mill for not less than 30 minutes to form the carbonaceous raw material.
8. The method for preparing a high-conductivity carbon electrode according to claim 4, wherein the binder comprises coal tar and polyimide, and the mass ratio of the coal tar to the polyimide is 1: (0.5-2).
9. The method for preparing a high-conductivity carbon electrode as claimed in claim 4, wherein the carbonaceous material and the binder are mixed uniformly and then placed into the mold, and the mixture is baked at 1200 ℃ and 1400 ℃ for 2-3h, and the baked material is naturally graphitized in a natural graphitization furnace at 2700 ℃ to 2900 ℃ for 40-50 h.
10. The method for preparing a high-conductivity carbon electrode according to claim 4, wherein the carbon fiber is prepared by chemical vapor deposition.
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